#------------------------------------------------------------------------------
#$Date: 2024-10-31 04:58:58 +0200 (Thu, 31 Oct 2024) $
#$Revision: 295687 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/26/2312674.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312674
loop_
_publ_author_name
'Steinke, Tim'
'Engelage, Elric'
'Huber, Stefan M.'
_publ_section_title
;
Chalcogen bonding in the solid-state structures of
1,3-bis(benzimidazoliumyl)benzene-based chalcogen-bonding donors.
;
_journal_coeditor_code QW3003
_journal_issue 'Pt 2'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first 26
_journal_page_last 35
_journal_paper_doi 10.1107/S2053229622011536
_journal_volume 79
_journal_year 2023
_chemical_formula_iupac 'C24 H24 N4 Se2 2+, 2C F3 O3 S -, 0.5C2 H4 Cl2'
_chemical_formula_moiety
'C24 H24 N4 Se2 2+, 2(C F3 O3 S -), 0.5(C2 H4 Cl2)'
_chemical_formula_sum 'C27 H26 Cl F6 N4 O6 S2 Se2'
_chemical_formula_weight 874.01
_chemical_name_systematic
;
3,3'-Bis(methylselanyl)-1,1'-(1,3-phenylene)bis(1H-1,3-benzodiazol-3-ium)
bis(trifluoromethanesulfonate) 1,2-dichloroethane hemisolvate
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_Hall '-P 1'
_space_group_name_H-M_alt 'P -1'
_atom_sites_solution_hydrogens geom
_audit_creation_method SHELXL-2018/3
_cell_angle_alpha 102.5150(10)
_cell_angle_beta 93.2310(10)
_cell_angle_gamma 96.1980(10)
_cell_formula_units_Z 2
_cell_length_a 9.36720(10)
_cell_length_b 13.3265(2)
_cell_length_c 13.64450(10)
_cell_measurement_reflns_used 5795
_cell_measurement_temperature 170(2)
_cell_measurement_theta_max 66.5
_cell_measurement_theta_min 3.3
_cell_volume 1647.49(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
DIAMOND (Putz & Brandenburg, 2014) and Mercury (Macrae et al.,
2020)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a) and shelXle (H\"ubschle et al.,
2011)
;
_diffrn_ambient_temperature 170.00(10)
_diffrn_detector 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device 'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku XtaLAB Synergy Dualflex diffractometer with a HyPix detector'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_monochromator mirror
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Cu K\a'
_diffrn_radiation_wavelength 1.54184
_diffrn_reflns_av_R_equivalents 0.0462
_diffrn_reflns_av_unetI/netI 0.0435
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 16
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 19605
_diffrn_reflns_theta_full 66.498
_diffrn_reflns_theta_max 66.498
_diffrn_reflns_theta_min 3.329
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 5.478
_exptl_absorpt_correction_T_max 1.000
_exptl_absorpt_correction_T_min 0.456
_exptl_absorpt_correction_type gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2018)
;
_exptl_crystal_colour 'translucent colourless'
_exptl_crystal_density_diffrn 1.762
_exptl_crystal_description 'cut plate'
_exptl_crystal_F_000 870
_exptl_crystal_size_max 0.189
_exptl_crystal_size_mid 0.096
_exptl_crystal_size_min 0.078
_refine_diff_density_max 0.841
_refine_diff_density_min -0.795
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.052
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 484
_refine_ls_number_reflns 5795
_refine_ls_number_restraints 28
_refine_ls_restrained_S_all 1.053
_refine_ls_R_factor_all 0.0513
_refine_ls_R_factor_gt 0.0480
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+3.3756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1244
_refine_ls_wR_factor_ref 0.1272
_reflns_number_gt 5307
_reflns_number_total 5795
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file qw3003.cif
_cod_data_source_block TS-056_3Se-C
_cod_database_code 2312674
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_hkl_file
;
0 0 1 16389.3 906.133 12
0 0 2 4986.33 323.368 10
0 0 3 570114. 29584.8 10
0 0 4 54924.2 2989.21 10
0 0 5 181497. 9582.19 10
0 0 6 906.933 124.398 15
0 0 6 1041.26 196.874 10
0 0 7 2556.71 328.108 10
0 0 7 2150.81 218.342 15
0 0 8 4096.08 460.853 10
0 0 8 3694.18 322.684 15
0 0 9 14999.0 879.644 19
0 0 9 15151.2 933.053 34
0 0 9 15069.3 944.100 15
0 0 9 15621.1 896.498 32
0 0 9 12419.5 1082.45 10
0 0 10 7856.38 496.217 19
0 0 10 6550.95 524.682 28
0 0 10 6897.56 521.220 40
0 0 10 7479.32 549.020 34
0 0 11 167.691 123.635 28
0 0 11 124.371 101.495 40
0 0 11-14.7794 94.4587 19
0 0 11-48.8925 124.045 34
0 0 12 8191.99 644.598 41
0 0 12 8554.40 653.978 28
0 0 12 10063.5 603.007 19
0 0 13 2443.44 284.670 41
0 0 13 3252.77 267.763 19
0 0 13 2644.51 259.885 27
0 0 13 3225.43 328.321 28
0 0 14 4014.94 416.462 16
0 0 14 4190.56 384.059 28
0 0 14 4642.29 347.997 27
0 0 14 5301.27 351.836 19
0 0 15 5463.31 336.428 19
0 0 15 5034.90 336.175 27
0 -1 16 2839.12 230.466 27
0 -1 16 3694.35 234.777 19
0 -1 16 3355.86 262.532 30
0 -1 15 6135.67 394.889 19
0 -1 15 6186.36 410.383 27
0 -1 15 5483.54 415.297 28
0 -1 14 4896.24 344.293 19
0 -1 14 4054.00 364.212 28
0 -1 14 4390.34 349.447 27
0 -1 13 374.569 125.379 28
0 -1 13 598.989 199.125 16
0 -1 13 575.816 137.209 19
0 -1 12 117.007 137.801 16
0 -1 12-79.4802 104.840 19
0 -1 12 45.3243 97.8488 28
0 -1 12 33.0688 98.5287 37
0 -1 12 87.4649 94.4125 41
0 -1 11 93.0109 96.0322 37
0 -1 11 143.305 106.313 19
0 -1 11 128.531 103.154 40
0 -1 11 236.674 105.569 28
0 -1 11 99.6274 117.542 34
0 -1 11 106.524 146.471 16
0 -1 10 817.939 154.164 40
0 -1 10 939.343 145.280 39
0 -1 10 848.389 143.119 19
0 -1 10 510.773 169.935 16
0 -1 10 621.626 156.063 34
0 -1 10 697.823 137.460 37
0 -1 10 914.315 154.195 28
0 -1 9 71712.4 3756.28 39
0 -1 9 67073.1 3810.75 34
0 -1 9 69002.3 3819.32 16
0 -1 9 70541.4 3759.27 37
0 -1 9 70025.3 3767.26 19
0 -1 9 77230.0 3770.59 26
0 -1 9 67160.8 3774.73 32
0 -1 8 1049.08 161.690 16
0 -1 8 876.680 157.563 15
0 -1 8 1030.43 231.954 10
0 -1 7 7500.62 489.124 16
0 -1 7 7042.35 492.693 15
0 -1 7 7848.68 650.041 10
0 -1 6 62300.6 3351.06 15
0 -1 6 63944.7 3518.37 10
0 -1 6 63069.8 3345.65 16
0 -1 5 53813.7 2998.83 10
0 -1 4 43355.2 2645.88 12
0 -1 4 52683.7 2627.99 10
0 1 -4 46840.6 2464.95 2
0 -1 4 46999.7 2470.65 8
0 1 -3 29164.6 1526.25 2
0 -1 3 27350.2 1640.27 12
0 -1 3 28144.6 1610.26 10
0 -1 2 4561.01 320.048 10
0 -1 2 4154.34 331.107 1
0 1 -2 4390.27 288.289 2
0 1 -1 89823.3 4163.78 9
0 1 -1 80064.4 4194.49 2
0 -1 0 8067.82 539.217 1
0 -1 -1 15507.4 1003.95 1
0 1 1 15901.7 947.234 2
0 1 1 18996.4 938.918 13
0 1 1 17052.9 946.036 12
0 1 2 98382.7 5408.72 12
0 1 2 101060. 5342.19 2
0 1 2 112345. 5426.90 13
0 -1 -2 101015. 5404.38 1
0 1 3 120166. 6104.08 2
0 -1 -3 114180. 6112.19 8
0 1 3 116926. 6251.73 12
0 1 4 180442. 9563.25 12
0 1 5 63639.7 3489.44 10
0 1 6 1102.59 135.141 14
0 1 6 1447.03 228.152 10
0 1 7 4644.63 360.415 16
0 1 7 4844.26 484.889 10
0 1 8 4914.08 544.925 10
0 1 8 5167.96 405.000 16
0 1 9 4964.82 360.744 19
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0 1 9 4970.08 430.883 15
0 1 9 5964.84 385.538 37
0 1 9 5339.09 429.604 16
0 1 9 4695.37 551.832 10
0 1 10 34635.1 2118.16 28
0 1 10 34779.0 2080.38 40
0 1 10 38169.4 2151.56 15
0 1 10 38383.3 2145.72 16
0 1 10 38495.4 2118.82 34
0 1 10 39324.7 2047.95 19
0 1 11 42860.6 2613.79 28
0 1 11 45953.1 2638.04 16
0 1 11 51169.9 2542.98 19
0 1 11 44480.7 2573.93 40
0 1 12 10828.6 612.749 19
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0 1 12 8372.47 593.094 27
0 1 12 8415.33 668.639 28
0 1 12 9515.32 703.053 16
0 1 13 8065.52 505.807 19
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0 1 13 7820.20 507.647 27
0 1 13 7140.67 587.365 16
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0 1 14 154.106 81.5036 27
0 1 14 231.701 97.1771 19
0 1 14 54.5463 74.8823 41
0 1 14 21.0213 110.415 28
0 1 15 320.898 78.5689 27
0 1 15 335.861 110.827 28
0 -2 16 613.510 89.9564 19
0 -2 16 332.397 106.613 30
0 -2 16 584.494 101.797 27
0 -2 15 383.774 113.391 27
0 -2 15 274.628 88.2753 19
0 -2 14 8256.61 641.323 16
0 -2 14 7661.89 543.208 27
0 -2 14 8602.49 539.972 19
0 -2 14 8243.23 559.169 28
0 -2 13 62.5925 95.5766 19
0 -2 13-19.2968 75.0008 28
0 -2 13 98.4244 102.547 37
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0 -2 2 97845.0 6004.67 1
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0 2 1 64856.5 3511.70 2
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0 2 2 178217. 9599.76 2
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0 -2 -2 183253. 9744.72 1
0 2 3 65408.0 3430.35 12
0 2 3 61778.6 3345.59 2
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0 -2 -4 196324. 10209.3 8
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0 2 6 62945.7 3423.80 10
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0 2 7 274213. 13840.3 16
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0 2 8 35639.2 1965.65 16
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0 2 8 34933.1 1939.92 34
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0 2 12 15518.8 1023.40 41
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0 2 15 1711.25 162.589 30
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0 -3 13 2796.40 268.188 19
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0 -3 13 2514.36 257.991 28
0 -3 12 21184.6 1235.78 19
0 -3 12 21052.8 1306.52 16
0 -3 12 19791.1 1222.53 28
0 -3 12 22196.8 1234.98 37
0 -3 11 35667.9 1915.95 19
0 -3 11 34445.9 1961.48 34
0 -3 11 33449.5 1893.29 37
0 -3 11 33916.0 1963.60 16
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0 -3 10 6200.66 431.112 37
0 -3 10 5964.17 454.949 32
0 -3 10 7055.31 494.324 40
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0 -3 8 123157. 6495.73 16
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0 -3 6 12719.1 828.936 8
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0 -3 3 42899.8 2668.28 1
0 3 -2 78275.9 4248.30 2
0 -3 1 19618.4 1365.86 1
0 -3 0 143477. 7805.40 1
0 -3 -1 19902.2 1381.18 1
0 3 1 19947.2 1207.84 2
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0 3 2 26542.3 1417.46 2
0 -3 -2 25007.3 1593.64 1
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0 -3 -4 727.699 146.308 8
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0 3 8 26889.0 1831.91 10
0 3 8 28502.3 1642.48 15
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0 3 8 27116.8 1582.01 34
0 3 8 28677.7 1627.47 14
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0 3 9 330.406 128.200 16
0 3 9 174.647 81.5882 27
0 3 9 289.661 86.8345 19
0 3 9 227.977 127.693 28
0 3 9 286.172 104.638 34
0 3 10 5687.49 411.972 27
0 3 10 6183.00 501.153 28
0 3 10 6209.56 417.321 19
0 3 10 6218.47 486.264 16
0 3 11 17617.9 1149.18 41
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0 4 -6 20739.3 1274.30 2
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0 -4 6 21394.5 1167.53 16
0 4 -5 7960.31 608.805 2
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0 4 -3 407692. 21158.0 2
0 -4 3 397440. 21409.1 1
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0 4 8 5049.97 428.546 14
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0 4 9 25459.3 1517.39 15
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-10 -5 4 1090.45 129.330 26
-10 -5 4 1023.17 134.290 23
-10 -5 4 1015.07 155.386 18
-10 -5 3 2178.21 220.429 17
-10 -5 3 1552.47 168.238 26
-10 -5 3 1739.70 176.699 23
-10 -5 3 2274.38 213.776 18
-10 -5 2 1526.11 161.678 23
-10 -5 2 1425.50 174.769 18
-10 -5 1 669.467 104.125 23
-10 -5 1 802.469 114.933 38
-10 -5 1 754.845 117.455 18
-10 -5 0 4017.93 294.989 38
-11 4 2 2931.71 254.315 24
-11 4 1 724.042 125.015 24
-11 4 1 556.135 109.072 23
-11 4 0 328.696 94.9982 24
-11 4 0 316.632 96.9221 23
-11 4 -1 2177.99 203.189 24
-11 4 -1 2029.68 207.111 23
-11 3 3 1209.85 154.359 24
-11 3 3 949.407 142.868 23
-11 3 3 1037.11 162.902 18
-11 3 2 238.489 91.3421 24
-11 3 2 205.368 97.4274 23
-11 3 1 111.428 83.2699 24
-11 3 1 158.757 100.564 23
-11 3 0 410.790 100.294 24
-11 3 0 348.477 116.593 23
-11 3 -1 72.0775 76.0804 24
-11 3 -1 133.752 99.7426 23
-11 2 3 6192.36 410.909 24
-11 2 3 5106.58 410.017 23
-11 2 2 183.988 84.8033 24
-11 2 2 155.036 105.558 23
-11 2 1 5170.59 376.865 24
-11 2 1 5058.98 409.730 23
-11 2 0 1227.84 158.305 24
-11 2 0 1406.64 202.472 23
-11 2 -1 2690.30 230.608 24
-11 2 -1 2944.81 290.555 23
-11 2 -2 1038.31 119.657 24
-11 2 -2 1322.62 186.465 23
-11 1 3 55.2054 76.9367 24
-11 1 3-17.2585 98.9143 23
-11 1 2 8845.00 571.221 24
-11 1 1 5825.32 409.806 24
-11 1 0 25.0483 65.7099 24
-11 1 -1 1076.94 129.984 24
-11 0 3 3434.84 280.504 24
-11 0 2 2743.47 243.407 24
-11 0 2 2735.78 274.656 23
-11 0 1-51.3948 70.6286 24
-11 0 1-37.0715 104.809 23
-11 0 0 825.930 161.382 23
-11 0 -1 35.2208 98.1738 23
-11 -1 2 277.494 107.509 23
-11 -1 1 147.027 106.904 23
0 0 0 0.00 0.00 0
;
_shelx_hkl_checksum 50439
_shelx_res_file
;
TITL shelxt_a.res in P-1
TS-056subm.res
created by SHELXL-2018/3 at 22:36:56 on 28-Oct-2022
REM Old TITL TS-056 in P-1
REM SHELXT solution in P-1: R1 0.131, Rweak 0.008, Alpha 0.052
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C28 N4 O5 F6 S3 Br2
CELL 1.54184 9.3672 13.3265 13.6445 102.515 93.231 96.198
ZERR 2.000 0.0001 0.0002 0.0001 0.001 0.001 0.001
LATT 1
SFAC C N O F S Cl Se H
UNIT 54 8 12 12 4 2 4 52
EADP C1B C1A
EADP C10A C10B
EADP S2A S2B
EADP O4A O4B O6A O6B O5A O5B
EXYZ O4A O4B
EADP C5A C5B
EADP C6A C6B
EADP C7A C7B
EADP C8A C8B
EADP C9A C9B
EADP SE1B SE1A
EADP C3A C3B
EADP N1A N1B
EADP N2A N2B
EADP C27A C27B
EADP C4A C4B
SADI SE1A C3A SE1B C3B
SADI N1A C4A N1B C4B
SADI N1A C3A N1B C3B
SADI N2A C3A N2B C3B
SADI N2A N1A N2B N1B
SADI N1A C5A n1B C5B
SADI C10A C5A C10B C5B
SADI N2A C10A N2B C10B
SADI C5A C6A C5B C6B
SADI C6A C7A C6B C7B
SADI C7A C8A C7B C8B
SADI C9A C10A C9B C10B
SADI C9A C8A C9B C8B
SADI C1A SE1A C1B Se1B
SADI C19 N2A C19 N2B
SADi C9A C6A C9B C6B
SADi C8A C6A C8B C6B
SADI C5A C8A C5B C8B
SADI C10A C7A C10B C7B
SADi N2B C4B N2A C4A
SADi C3B C4B C3A C4A
SADI S2A O4A S2A O5A S2A O6A
SADI S2A C26 S2B C26
SADI S2B O4B S2B O5B S2B O6B
L.S. 100
BOND $H
temp -103
LIST 6
omit -3 133
acta
FMAP 2
PLAN 20
WGHT 0.060700 3.375600
FVAR 3.90301 0.94980 0.57370 0.48027
Part 1
SE1A 7 0.512288 0.780776 0.206626 21.00000 0.04029 0.03396 =
0.03875 0.01247 0.00641 0.00902
N1A 2 0.362893 0.766446 0.382227 21.00000 0.03853 0.03130 =
0.02351 -0.00164 0.00218 0.01214
N2A 2 0.414632 0.616201 0.303995 21.00000 0.02569 0.02706 =
0.02440 0.00123 0.00292 0.00701
C1A 1 0.703676 0.737927 0.216629 21.00000 0.03391 0.05156 =
0.04130 0.01043 0.00571 0.00683
AFIX 137
H1AA 8 0.764582 0.768208 0.171733 21.00000 -1.50000
H1AB 8 0.696569 0.662222 0.196995 21.00000 -1.50000
H1AC 8 0.746273 0.761771 0.286196 21.00000 -1.50000
AFIX 0
C3A 1 0.427701 0.717256 0.304146 21.00000 0.03121 0.02959 =
0.02310 0.00201 -0.00012 0.00955
C4A 1 0.351543 0.877368 0.409782 21.00000 0.07217 0.03281 =
0.04450 -0.00041 0.01280 0.02039
AFIX 137
H4AA 8 0.360353 0.900770 0.483322 21.00000 -1.50000
H4AB 8 0.257903 0.890591 0.382867 21.00000 -1.50000
H4AC 8 0.428760 0.915132 0.381636 21.00000 -1.50000
AFIX 0
SAME C5A > C10A
C5A 1 0.302661 0.694334 0.432347 21.00000 0.03625 0.03606 =
0.02051 0.00088 -0.00019 0.00993
C6A 1 0.216051 0.704140 0.513759 21.00000 0.04732 0.05233 =
0.02606 -0.00092 0.00649 0.01837
AFIX 43
H6A 8 0.190937 0.769239 0.547424 21.00000 -1.20000
AFIX 0
C7A 1 0.169625 0.613413 0.541892 21.00000 0.05231 0.05924 =
0.02574 0.00758 0.01135 0.01057
AFIX 43
H7A 8 0.108846 0.616114 0.595601 21.00000 -1.20000
AFIX 0
C8A 1 0.208684 0.518031 0.494363 21.00000 0.04201 0.05556 =
0.03034 0.01387 0.00521 0.00327
AFIX 43
H8A 8 0.176484 0.458318 0.518278 21.00000 -1.20000
AFIX 0
C9A 1 0.292400 0.507448 0.413889 21.00000 0.03526 0.04263 =
0.02611 0.00803 0.00589 0.01031
AFIX 43
H9A 8 0.317749 0.442275 0.380633 21.00000 -1.20000
AFIX 0
C10A 1 0.337346 0.598651 0.384577 21.00000 0.02634 0.03495 =
0.02190 0.00201 -0.00164 0.00756
Part 2
SE1B 7 0.352045 0.467862 0.449218 -21.00000 0.04029 0.03396 =
0.03875 0.01247 0.00641 0.00902
C1B 1 0.169501 0.503138 0.498570 -21.00000 0.03391 0.05156 =
0.04130 0.01043 0.00571 0.00683
AFIX 137
H1BA 8 0.154002 0.571836 0.488350 -21.00000 -1.50000
H1BB 8 0.171045 0.503692 0.570562 -21.00000 -1.50000
H1BC 8 0.091254 0.451706 0.461725 -21.00000 -1.50000
AFIX 0
N1B 2 10.314376 10.678949 10.447267 -21.00000 0.03853 0.03130 =
0.02351 -0.00164 0.00218 0.01214
N2B 2 0.407639 0.604370 0.312301 -21.00000 0.02569 0.02706 =
0.02440 0.00123 0.00292 0.00701
C3B 1 0.358791 0.590467 0.399929 -21.00000 0.03121 0.02959 =
0.02310 0.00201 -0.00012 0.00955
C4B 1 0.261529 0.702413 0.546934 -21.00000 0.07217 0.03281 =
0.04450 -0.00041 0.01280 0.02039
AFIX 137
H4BA 8 0.267257 0.777660 0.571149 -21.00000 -1.50000
H4BB 8 0.320596 0.674078 0.593420 -21.00000 -1.50000
H4BC 8 0.161140 0.671305 0.543359 -21.00000 -1.50000
AFIX 0
SAME C5B > C10B
C5B 1 0.341085 0.761780 0.402765 -21.00000 0.03625 0.03606 =
0.02051 0.00088 -0.00019 0.00993
C6B 1 0.322205 0.867139 0.416635 -21.00000 0.04732 0.05233 =
0.02606 -0.00092 0.00649 0.01837
AFIX 43
H6B 8 0.282495 0.904160 0.474158 -21.00000 -1.20000
AFIX 0
C7B 1 0.366122 0.911894 0.339853 -21.00000 0.05231 0.05924 =
0.02574 0.00758 0.01135 0.01057
AFIX 43
H7B 8 0.340495 0.978647 0.338420 -21.00000 -1.20000
AFIX 0
C8B 1 0.446477 0.864318 0.263823 -21.00000 0.04201 0.05556 =
0.03034 0.01387 0.00521 0.00327
AFIX 43
H8B 8 0.482276 0.901547 0.216517 -21.00000 -1.20000
AFIX 0
C9B 1 0.474153 0.763473 0.257056 -21.00000 0.03526 0.04263 =
0.02611 0.00803 0.00589 0.01031
AFIX 43
H9B 8 0.532521 0.731073 0.207871 -21.00000 -1.20000
AFIX 0
C10B 1 0.413388 0.711764 0.324807 -21.00000 0.02634 0.03495 =
0.02190 0.00201 -0.00164 0.00756
Part 0
C2A 1 0.957745 0.580880 0.277481 11.00000 0.04616 0.04200 =
0.04053 0.00675 -0.00021 -0.00253
AFIX 137
H2AA 8 1.000622 0.651134 0.276882 11.00000 -1.50000
H2AB 8 1.022288 0.549576 0.317907 11.00000 -1.50000
H2AC 8 0.864711 0.583860 0.306753 11.00000 -1.50000
AFIX 0
N3 2 0.721124 0.346597 0.193556 11.00000 0.03145 0.02617 =
0.02753 0.00471 0.00573 0.01032
N4 2 0.936137 0.297789 0.191553 11.00000 0.03210 0.03474 =
0.02704 0.00466 0.00314 0.01060
SE2 7 0.928960 0.496971 0.139198 11.00000 0.03739 0.03488 =
0.03539 0.01026 0.00790 0.00516
C11 1 0.859726 0.372664 0.176934 11.00000 0.03190 0.03285 =
0.02340 0.00338 0.00346 0.01084
C12 1 1.089416 0.292361 0.176877 11.00000 0.03116 0.05557 =
0.04011 0.01291 0.00521 0.01660
AFIX 137
H12A 8 1.139658 0.284118 0.239078 11.00000 -1.50000
H12B 8 1.131541 0.356278 0.159712 11.00000 -1.50000
H12C 8 1.099365 0.233066 0.122044 11.00000 -1.50000
AFIX 0
C13 1 0.845312 0.219072 0.216571 11.00000 0.03842 0.03202 =
0.02280 0.00207 0.00529 0.00984
C14 1 0.872399 0.125665 0.239496 11.00000 0.05160 0.03542 =
0.03247 0.00751 0.00409 0.01766
AFIX 43
H14 8 0.965944 0.104311 0.238527 11.00000 -1.20000
AFIX 0
C15 1 0.756093 0.066026 0.263631 11.00000 0.06296 0.03011 =
0.04161 0.00829 0.00524 0.01321
AFIX 43
H15 8 0.769564 0.001151 0.278621 11.00000 -1.20000
AFIX 0
C16 1 0.618093 0.098083 0.266794 11.00000 0.05866 0.03270 =
0.04305 0.00960 0.01012 0.00370
AFIX 43
H16 8 0.541410 0.054914 0.285092 11.00000 -1.20000
AFIX 0
C17 1 0.590573 0.191302 0.243873 11.00000 0.04149 0.03586 =
0.03859 0.00660 0.01070 0.00754
AFIX 43
H17 8 0.497432 0.213314 0.245928 11.00000 -1.20000
AFIX 0
C18 1 0.708236 0.250254 0.217738 11.00000 0.03750 0.02828 =
0.02735 0.00347 0.00431 0.00979
C19 1 0.453744 0.533653 0.227273 11.00000 0.02739 0.02562 =
0.02398 0.00160 0.00576 0.00519
C20 1 0.372911 0.506156 0.135515 11.00000 0.03007 0.03596 =
0.03068 0.00507 0.00122 0.01150
AFIX 43
H20 8 0.295222 0.542871 0.122199 11.00000 -1.20000
AFIX 0
C21 1 0.407550 0.423737 0.063131 11.00000 0.04275 0.04452 =
0.02566 -0.00025 -0.00309 0.01383
AFIX 43
H21 8 0.351792 0.402888 0.000176 11.00000 -1.20000
AFIX 0
C22 1 0.522807 0.371684 0.082029 11.00000 0.04245 0.03196 =
0.02333 -0.00086 0.00332 0.01011
AFIX 43
H22 8 0.547201 0.315945 0.032132 11.00000 -1.20000
AFIX 0
C23 1 0.602050 0.402093 0.174799 11.00000 0.03066 0.02733 =
0.02782 0.00721 0.00795 0.00830
C24 1 0.567821 0.482064 0.249782 11.00000 0.02994 0.02653 =
0.02381 0.00297 0.00285 0.00557
AFIX 43
H24 8 0.620428 0.500739 0.313983 11.00000 -1.20000
AFIX 0
S1 5 0.118189 0.754683 0.095792 11.00000 0.03574 0.03504 =
0.03032 0.00643 0.00675 0.01252
F1 4 0.208792 0.948940 0.175962 11.00000 0.08281 0.05580 =
0.10042 -0.01679 0.03181 -0.01947
F2 4 -0.003876 0.899839 0.208168 11.00000 0.08048 0.05783 =
0.13697 -0.01494 0.06504 0.01516
F3 4 0.035637 0.924558 0.061617 11.00000 0.11667 0.07840 =
0.15785 0.06860 0.00220 0.04104
O1 3 0.176465 0.731614 0.187135 11.00000 0.05147 0.08010 =
0.04646 0.03106 0.00521 0.01983
O2 3 0.218873 0.758525 0.020646 11.00000 0.05094 0.06422 =
0.03271 0.00423 0.01397 0.01237
O3 3 -0.022679 0.700837 0.059941 11.00000 0.04964 0.05230 =
0.05154 0.00686 -0.00178 -0.00280
C25 1 0.087854 0.889508 0.136957 11.00000 0.05436 0.04562 =
0.07971 0.01170 0.02068 0.00932
F4 4 0.043668 0.167021 0.541275 11.00000 0.06525 0.09750 =
0.19771 -0.01188 0.05120 0.00321
F5 4 0.209021 0.078571 0.559061 11.00000 0.14854 0.06172 =
0.06342 0.02371 -0.00802 0.00824
F6 4 0.093731 0.053096 0.414556 11.00000 0.09153 0.05385 =
0.07945 0.00376 -0.02694 -0.00895
C26 1 0.148254 0.125978 0.495032 11.00000 0.04966 0.04245 =
0.06661 -0.00271 -0.00441 0.01075
PART 1
CL1A 6 0.351779 0.108783 -0.012102 31.00000 0.07179 0.05644 =
0.05657 0.01561 0.00820 -0.00223
C27A 1 0.513566 0.049010 -0.018353 31.00000 0.05381 0.04787 =
0.04813 0.00916 0.00818 -0.00605
AFIX 23
H27A 8 0.540977 0.033300 -0.088571 31.00000 -1.20000
H27B 8 0.593142 0.096079 0.024336 31.00000 -1.20000
AFIX 0
PART 2
CL1B 6 0.345478 0.110585 0.002606 -31.00000 0.06110 0.06327 =
0.07750 0.01459 0.01287 0.01606
C27B 1 0.422846 -0.005121 0.014059 -31.00000 0.05381 0.04787 =
0.04813 0.00916 0.00818 -0.00605
AFIX 23
H27C 8 0.420525 -0.014172 0.084101 -31.00000 -1.20000
H27D 8 0.366556 -0.066503 -0.031233 -31.00000 -1.20000
AFIX 0
PART 0
Part 1
S2A 5 0.259355 0.231146 0.463928 41.00000 0.04384 0.05304 =
0.03369 0.00999 0.00189 0.00478
O4A 3 0.316645 0.296646 0.552656 41.00000 0.06820 0.06755 =
0.05268 0.01890 -0.01075 -0.00370
O5A 3 0.160385 0.265894 0.400381 41.00000 0.06820 0.06755 =
0.05268 0.01890 -0.01075 -0.00370
O6A 3 0.373113 0.179586 0.415991 41.00000 0.06820 0.06755 =
0.05268 0.01890 -0.01075 -0.00370
Part 2
S2B 5 0.296706 0.210890 0.459604 -41.00000 0.04384 0.05304 =
0.03369 0.00999 0.00189 0.00478
O4B 3 0.316645 0.296646 0.552656 -41.00000 0.06820 0.06755 =
0.05268 0.01890 -0.01075 -0.00370
O5B 3 0.244706 0.242917 0.372131 -41.00000 0.06820 0.06755 =
0.05268 0.01890 -0.01075 -0.00370
O6B 3 0.403548 0.139185 0.442992 -41.00000 0.06820 0.06755 =
0.05268 0.01890 -0.01075 -0.00370
Part 0
HKLF 4
REM shelxt_a.res in P-1
REM wR2 = 0.1272, GooF = S = 1.052, Restrained GooF = 1.053 for all data
REM R1 = 0.0480 for 5307 Fo > 4sig(Fo) and 0.0513 for all 5795 data
REM 484 parameters refined using 28 restraints
END
WGHT 0.0607 3.3617
REM Highest difference peak 0.841, deepest hole -0.795, 1-sigma level 0.092
Q1 1 0.0480 0.2058 0.4747 11.00000 0.05 0.84
Q2 1 0.2348 0.2779 0.4622 11.00000 0.05 0.77
Q3 1 0.3209 0.2438 0.3665 11.00000 0.05 0.77
Q4 1 0.4414 0.1267 0.1685 11.00000 0.05 0.72
Q5 1 0.1271 0.1251 0.5684 11.00000 0.05 0.67
Q6 1 0.1039 0.2821 0.4282 11.00000 0.05 0.63
Q7 1 0.5019 0.7029 0.1791 11.00000 0.05 0.56
Q8 1 0.5150 0.8595 0.2295 11.00000 0.05 0.54
Q9 1 0.1032 0.8219 0.1186 11.00000 0.05 0.54
Q10 1 0.3550 0.1220 0.3983 11.00000 0.05 0.51
Q11 1 -0.0301 0.8984 0.1278 11.00000 0.05 0.49
Q12 1 0.9432 0.5769 0.1489 11.00000 0.05 0.48
Q13 1 0.9220 0.4230 0.1278 11.00000 0.05 0.47
Q14 1 0.3847 0.1066 0.4776 11.00000 0.05 0.45
Q15 1 0.2428 0.4598 0.3926 11.00000 0.05 0.44
Q16 1 0.0592 0.8918 0.0003 11.00000 0.05 0.43
Q17 1 0.4787 0.7243 0.2607 11.00000 0.05 0.40
Q18 1 0.4293 0.1834 0.4558 11.00000 0.05 0.37
Q19 1 0.2890 0.5395 0.3813 11.00000 0.05 0.35
Q20 1 0.3052 0.0987 0.5192 11.00000 0.05 0.33
;
_shelx_res_checksum 67992
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Se Se1A 0.51229(5) 0.78078(3) 0.20663(3) 0.03655(15) Uani d 0.9498(10) A 1
N N1A 0.3629(6) 0.7664(3) 0.3822(3) 0.0317(8) Uani d 0.9498(10) A 1
N N2A 0.4146(11) 0.6162(3) 0.3040(4) 0.0261(7) Uani d 0.9498(10) A 1
C C1A 0.7037(5) 0.7379(4) 0.2166(3) 0.0420(10) Uani d 0.9498(10) A 1
H H1AA 0.764582 0.768208 0.171733 0.063 Uiso calc 0.9498(10) A 1
H H1AB 0.696569 0.662222 0.196995 0.063 Uiso calc 0.9498(10) A 1
H H1AC 0.746273 0.761771 0.286196 0.063 Uiso calc 0.9498(10) A 1
C C3A 0.4277(7) 0.7173(3) 0.3041(3) 0.0282(10) Uani d 0.9498(10) A 1
C C4A 0.3515(9) 0.8774(4) 0.4098(6) 0.0499(17) Uani d 0.9498(10) A 1
H H4AA 0.360353 0.900770 0.483322 0.075 Uiso calc 0.9498(10) A 1
H H4AB 0.257903 0.890591 0.382867 0.075 Uiso calc 0.9498(10) A 1
H H4AC 0.428760 0.915132 0.381636 0.075 Uiso calc 0.9498(10) A 1
C C5A 0.3027(4) 0.6943(3) 0.4323(3) 0.0315(8) Uani d 0.9498(10) A 1
C C6A 0.2161(5) 0.7041(4) 0.5138(3) 0.0423(11) Uani d 0.9498(10) A 1
H H6A 0.190937 0.769239 0.547424 0.051 Uiso calc 0.9498(10) A 1
C C7A 0.1696(5) 0.6134(4) 0.5419(3) 0.0455(11) Uani d 0.9498(10) A 1
H H7A 0.108846 0.616114 0.595601 0.055 Uiso calc 0.9498(10) A 1
C C8A 0.2087(5) 0.5180(4) 0.4944(5) 0.0421(12) Uani d 0.9498(10) A 1
H H8A 0.176484 0.458318 0.518278 0.051 Uiso calc 0.9498(10) A 1
C C9A 0.2924(4) 0.5074(3) 0.4139(3) 0.0341(9) Uani d 0.9498(10) A 1
H H9A 0.317749 0.442275 0.380633 0.041 Uiso calc 0.9498(10) A 1
C C10A 0.3373(5) 0.5987(4) 0.3846(3) 0.0283(11) Uani d 0.9498(10) A 1
Se Se1B 0.3520(10) 0.4679(6) 0.4492(6) 0.03655(15) Uani d 0.0502(10) A 2
C C1B 0.170(9) 0.503(11) 0.499(13) 0.0420(10) Uani d 0.0502(10) A 2
H H1BA 0.154002 0.571836 0.488350 0.063 Uiso calc 0.0502(10) A 2
H H1BB 0.171045 0.503692 0.570562 0.063 Uiso calc 0.0502(10) A 2
H H1BC 0.091254 0.451706 0.461725 0.063 Uiso calc 0.0502(10) A 2
N N1B 0.314376 0.678949 0.447267 0.0317(8) Uani d 0.0502(10) A 2
N N2B 0.41(2) 0.604(4) 0.312(8) 0.0261(7) Uani d 0.0502(10) A 2
C C3B 0.359(15) 0.590(4) 0.400(5) 0.0282(10) Uani d 0.0502(10) A 2
C C4B 0.262(13) 0.702(6) 0.547(4) 0.0499(17) Uani d 0.0502(10) A 2
H H4BA 0.267257 0.777660 0.571149 0.075 Uiso calc 0.0502(10) A 2
H H4BB 0.320596 0.674078 0.593420 0.075 Uiso calc 0.0502(10) A 2
H H4BC 0.161140 0.671305 0.543359 0.075 Uiso calc 0.0502(10) A 2
C C5B 0.341(16) 0.762(5) 0.403(8) 0.0315(8) Uani d 0.0502(10) A 2
C C6B 0.322(19) 0.867(6) 0.417(9) 0.0423(11) Uani d 0.0502(10) A 2
H H6B 0.282495 0.904160 0.474158 0.051 Uiso calc 0.0502(10) A 2
C C7B 0.366(9) 0.912(4) 0.340(5) 0.0455(11) Uani d 0.0502(10) A 2
H H7B 0.340495 0.978647 0.338420 0.055 Uiso calc 0.0502(10) A 2
C C8B 0.446(8) 0.864(4) 0.264(4) 0.0421(12) Uani d 0.0502(10) A 2
H H8B 0.482276 0.901547 0.216517 0.051 Uiso calc 0.0502(10) A 2
C C9B 0.474(8) 0.763(4) 0.257(5) 0.0341(9) Uani d 0.0502(10) A 2
H H9B 0.532521 0.731073 0.207871 0.041 Uiso calc 0.0502(10) A 2
C C10B 0.413(16) 0.712(4) 0.325(8) 0.0283(11) Uani d 0.0502(10) A 2
C C2A 0.9577(5) 0.5809(3) 0.2775(3) 0.0440(10) Uani d 1 . .
H H2AA 1.000622 0.651134 0.276882 0.066 Uiso calc 1 . .
H H2AB 1.022288 0.549576 0.317907 0.066 Uiso calc 1 . .
H H2AC 0.864711 0.583860 0.306753 0.066 Uiso calc 1 . .
N N3 0.7211(3) 0.3466(2) 0.1936(2) 0.0279(6) Uani d 1 . .
N N4 0.9361(3) 0.2978(2) 0.1916(2) 0.0311(6) Uani d 1 . .
Se Se2 0.92896(4) 0.49697(3) 0.13920(3) 0.03528(14) Uani d 1 . .
C C11 0.8597(4) 0.3727(3) 0.1769(3) 0.0293(7) Uani d 1 . .
C C12 1.0894(4) 0.2924(4) 0.1769(3) 0.0410(9) Uani d 1 . .
H H12A 1.139658 0.284118 0.239078 0.062 Uiso calc 1 . .
H H12B 1.131541 0.356278 0.159712 0.062 Uiso calc 1 . .
H H12C 1.099365 0.233066 0.122044 0.062 Uiso calc 1 . .
C C13 0.8453(4) 0.2191(3) 0.2166(3) 0.0312(8) Uani d 1 . .
C C14 0.8724(5) 0.1257(3) 0.2395(3) 0.0389(9) Uani d 1 . .
H H14 0.965944 0.104311 0.238527 0.047 Uiso calc 1 . .
C C15 0.7561(5) 0.0660(3) 0.2636(3) 0.0443(10) Uani d 1 . .
H H15 0.769564 0.001151 0.278621 0.053 Uiso calc 1 . .
C C16 0.6181(5) 0.0981(3) 0.2668(3) 0.0445(10) Uani d 1 . .
H H16 0.541410 0.054914 0.285092 0.053 Uiso calc 1 . .
C C17 0.5906(5) 0.1913(3) 0.2439(3) 0.0384(9) Uani d 1 . .
H H17 0.497432 0.213314 0.245928 0.046 Uiso calc 1 . .
C C18 0.7082(4) 0.2503(3) 0.2177(3) 0.0310(8) Uani d 1 . .
C C19 0.4537(4) 0.5337(3) 0.2273(2) 0.0260(7) Uani d 1 . .
C C20 0.3729(4) 0.5062(3) 0.1355(3) 0.0321(8) Uani d 1 . .
H H20 0.295222 0.542871 0.122199 0.039 Uiso calc 1 . .
C C21 0.4075(5) 0.4237(3) 0.0631(3) 0.0385(9) Uani d 1 . .
H H21 0.351792 0.402888 0.000176 0.046 Uiso calc 1 . .
C C22 0.5228(4) 0.3717(3) 0.0820(3) 0.0332(8) Uani d 1 . .
H H22 0.547201 0.315945 0.032132 0.040 Uiso calc 1 . .
C C23 0.6021(4) 0.4021(3) 0.1748(3) 0.0279(7) Uani d 1 . .
C C24 0.5678(4) 0.4821(3) 0.2498(3) 0.0270(7) Uani d 1 . .
H H24 0.620428 0.500739 0.313983 0.032 Uiso calc 1 . .
S S1 0.11819(10) 0.75468(7) 0.09579(7) 0.0331(2) Uani d 1 . .
F F1 0.2088(4) 0.9489(3) 0.1760(3) 0.0861(12) Uani d 1 . .
F F2 -0.0039(4) 0.8998(3) 0.2082(3) 0.0947(14) Uani d 1 . .
F F3 0.0356(5) 0.9246(3) 0.0616(4) 0.1094(15) Uani d 1 . .
O O1 0.1765(4) 0.7316(3) 0.1871(2) 0.0558(8) Uani d 1 . .
O O2 0.2189(3) 0.7585(3) 0.0206(2) 0.0495(8) Uani d 1 . .
O O3 -0.0227(4) 0.7008(3) 0.0599(2) 0.0528(8) Uani d 1 . .
C C25 0.0879(6) 0.8895(4) 0.1370(5) 0.0594(13) Uani d 1 . .
F F4 0.0437(4) 0.1670(4) 0.5413(5) 0.126(2) Uani d 1 . .
F F5 0.2090(5) 0.0786(3) 0.5591(3) 0.0908(12) Uani d 1 . .
F F6 0.0937(4) 0.0531(2) 0.4146(3) 0.0793(10) Uani d 1 . .
C C26 0.1483(5) 0.1260(4) 0.4950(4) 0.0552(12) Uani d 1 . .
Cl Cl1A 0.352(2) 0.1088(13) -0.0121(18) 0.062(2) Uani d 0.574(10) B 1
C C27A 0.5136(10) 0.0490(7) -0.0184(7) 0.0509(18) Uani d 0.574(10) B 1
H H27A 0.540977 0.033300 -0.088571 0.061 Uiso calc 0.574(10) B 1
H H27B 0.593142 0.096079 0.024336 0.061 Uiso calc 0.574(10) B 1
Cl Cl1B 0.345(3) 0.1106(19) 0.003(2) 0.067(5) Uani d 0.426(10) B 2
C C27B 0.4228(14) -0.0051(10) 0.0141(9) 0.0509(18) Uani d 0.426(10) B 2
H H27C 0.420525 -0.014172 0.084101 0.061 Uiso calc 0.426(10) B 2
H H27D 0.366556 -0.066503 -0.031233 0.061 Uiso calc 0.426(10) B 2
S S2A 0.2594(6) 0.2311(5) 0.4639(5) 0.0436(9) Uani d 0.480(4) C 1
O O4A 0.3166(4) 0.2966(3) 0.5527(3) 0.0635(7) Uani d 0.480(4) C 1
O O5A 0.1604(10) 0.2659(6) 0.4004(6) 0.0635(7) Uani d 0.480(4) C 1
O O6A 0.3731(9) 0.1796(7) 0.4160(6) 0.0635(7) Uani d 0.480(4) C 1
S S2B 0.2967(6) 0.2109(5) 0.4596(5) 0.0436(9) Uani d 0.520(4) C 2
O O4B 0.3166(4) 0.2966(3) 0.5527(3) 0.0635(7) Uani d 0.520(4) C 2
O O5B 0.2447(9) 0.2429(6) 0.3721(5) 0.0635(7) Uani d 0.520(4) C 2
O O6B 0.4035(8) 0.1392(6) 0.4430(6) 0.0635(7) Uani d 0.520(4) C 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Se1A 0.0403(3) 0.0340(2) 0.0387(3) 0.00902(18) 0.00641(19) 0.01247(18)
N1A 0.039(3) 0.0313(17) 0.024(2) 0.0121(15) 0.0022(16) -0.0016(14)
N2A 0.0257(19) 0.0271(16) 0.0244(18) 0.007(2) 0.0029(13) 0.0012(13)
C1A 0.034(2) 0.052(3) 0.041(2) 0.0068(19) 0.0057(18) 0.010(2)
C3A 0.031(2) 0.0296(19) 0.023(3) 0.0095(16) -0.0001(19) 0.0020(15)
C4A 0.072(6) 0.033(2) 0.045(3) 0.020(3) 0.013(3) 0.000(2)
C5A 0.036(2) 0.036(2) 0.0205(17) 0.0099(16) -0.0002(15) 0.0009(15)
C6A 0.047(3) 0.052(3) 0.0261(19) 0.018(2) 0.0065(18) -0.0009(19)
C7A 0.052(3) 0.059(3) 0.026(2) 0.011(2) 0.0114(18) 0.0076(19)
C8A 0.042(3) 0.056(3) 0.030(2) 0.003(3) 0.005(3) 0.014(2)
C9A 0.035(2) 0.043(2) 0.0261(18) 0.0103(18) 0.0059(16) 0.0080(17)
C10A 0.026(3) 0.035(2) 0.0219(19) 0.0076(15) -0.0016(18) 0.0020(15)
Se1B 0.0403(3) 0.0340(2) 0.0387(3) 0.00902(18) 0.00641(19) 0.01247(18)
C1B 0.034(2) 0.052(3) 0.041(2) 0.0068(19) 0.0057(18) 0.010(2)
N1B 0.039(3) 0.0313(17) 0.024(2) 0.0121(15) 0.0022(16) -0.0016(14)
N2B 0.0257(19) 0.0271(16) 0.0244(18) 0.007(2) 0.0029(13) 0.0012(13)
C3B 0.031(2) 0.0296(19) 0.023(3) 0.0095(16) -0.0001(19) 0.0020(15)
C4B 0.072(6) 0.033(2) 0.045(3) 0.020(3) 0.013(3) 0.000(2)
C5B 0.036(2) 0.036(2) 0.0205(17) 0.0099(16) -0.0002(15) 0.0009(15)
C6B 0.047(3) 0.052(3) 0.0261(19) 0.018(2) 0.0065(18) -0.0009(19)
C7B 0.052(3) 0.059(3) 0.026(2) 0.011(2) 0.0114(18) 0.0076(19)
C8B 0.042(3) 0.056(3) 0.030(2) 0.003(3) 0.005(3) 0.014(2)
C9B 0.035(2) 0.043(2) 0.0261(18) 0.0103(18) 0.0059(16) 0.0080(17)
C10B 0.026(3) 0.035(2) 0.0219(19) 0.0076(15) -0.0016(18) 0.0020(15)
C2A 0.046(2) 0.042(2) 0.041(2) -0.0025(18) -0.0002(18) 0.0067(18)
N3 0.0314(15) 0.0262(14) 0.0275(14) 0.0103(12) 0.0057(12) 0.0047(12)
N4 0.0321(16) 0.0347(16) 0.0270(15) 0.0106(13) 0.0031(12) 0.0047(12)
Se2 0.0374(2) 0.0349(2) 0.0354(2) 0.00516(17) 0.00790(17) 0.01026(17)
C11 0.0319(19) 0.0328(18) 0.0234(16) 0.0108(15) 0.0035(14) 0.0034(14)
C12 0.031(2) 0.056(2) 0.040(2) 0.0166(18) 0.0052(16) 0.0129(19)
C13 0.038(2) 0.0320(18) 0.0228(16) 0.0098(15) 0.0053(14) 0.0021(14)
C14 0.052(2) 0.035(2) 0.0325(19) 0.0177(18) 0.0041(17) 0.0075(16)
C15 0.063(3) 0.030(2) 0.042(2) 0.0132(19) 0.005(2) 0.0083(17)
C16 0.059(3) 0.033(2) 0.043(2) 0.0037(19) 0.010(2) 0.0096(17)
C17 0.041(2) 0.036(2) 0.039(2) 0.0075(17) 0.0107(17) 0.0066(17)
C18 0.037(2) 0.0283(18) 0.0274(17) 0.0098(15) 0.0043(15) 0.0035(14)
C19 0.0274(17) 0.0256(17) 0.0240(16) 0.0052(13) 0.0058(13) 0.0016(13)
C20 0.0301(18) 0.0360(19) 0.0307(18) 0.0115(15) 0.0012(14) 0.0051(15)
C21 0.043(2) 0.045(2) 0.0257(18) 0.0138(18) -0.0031(15) -0.0003(16)
C22 0.042(2) 0.0320(18) 0.0233(17) 0.0101(16) 0.0033(15) -0.0009(14)
C23 0.0307(18) 0.0273(17) 0.0278(17) 0.0083(14) 0.0079(14) 0.0072(14)
C24 0.0299(17) 0.0265(17) 0.0238(16) 0.0056(14) 0.0028(13) 0.0030(13)
S1 0.0357(5) 0.0350(5) 0.0303(4) 0.0125(4) 0.0068(4) 0.0064(4)
F1 0.083(2) 0.0558(18) 0.100(3) -0.0195(17) 0.032(2) -0.0168(18)
F2 0.080(2) 0.0578(19) 0.137(3) 0.0152(17) 0.065(2) -0.015(2)
F3 0.117(3) 0.078(3) 0.158(4) 0.041(2) 0.002(3) 0.069(3)
O1 0.0515(19) 0.080(2) 0.0465(17) 0.0198(17) 0.0052(14) 0.0311(17)
O2 0.0509(18) 0.064(2) 0.0327(15) 0.0124(15) 0.0140(13) 0.0042(14)
O3 0.0496(18) 0.0523(18) 0.0515(18) -0.0028(15) -0.0018(14) 0.0069(15)
C25 0.054(3) 0.046(3) 0.080(4) 0.009(2) 0.021(3) 0.012(3)
F4 0.065(2) 0.098(3) 0.198(5) 0.003(2) 0.051(3) -0.012(3)
F5 0.149(4) 0.062(2) 0.063(2) 0.008(2) -0.008(2) 0.0237(16)
F6 0.092(2) 0.0539(18) 0.079(2) -0.0090(17) -0.0269(19) 0.0038(16)
C26 0.050(3) 0.042(2) 0.067(3) 0.011(2) -0.004(2) -0.003(2)
Cl1A 0.072(5) 0.056(3) 0.057(3) -0.002(3) 0.008(3) 0.016(2)
C27A 0.054(5) 0.048(5) 0.048(3) -0.006(3) 0.008(4) 0.009(3)
Cl1B 0.061(4) 0.063(5) 0.078(12) 0.016(4) 0.013(5) 0.015(5)
C27B 0.054(5) 0.048(5) 0.048(3) -0.006(3) 0.008(4) 0.009(3)
S2A 0.044(3) 0.053(2) 0.0337(7) 0.0048(14) 0.0019(15) 0.0100(13)
O4A 0.0682(17) 0.0675(17) 0.0527(15) -0.0037(14) -0.0107(12) 0.0189(12)
O5A 0.0682(17) 0.0675(17) 0.0527(15) -0.0037(14) -0.0107(12) 0.0189(12)
O6A 0.0682(17) 0.0675(17) 0.0527(15) -0.0037(14) -0.0107(12) 0.0189(12)
S2B 0.044(3) 0.053(2) 0.0337(7) 0.0048(14) 0.0019(15) 0.0100(13)
O4B 0.0682(17) 0.0675(17) 0.0527(15) -0.0037(14) -0.0107(12) 0.0189(12)
O5B 0.0682(17) 0.0675(17) 0.0527(15) -0.0037(14) -0.0107(12) 0.0189(12)
O6B 0.0682(17) 0.0675(17) 0.0527(15) -0.0037(14) -0.0107(12) 0.0189(12)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 2 0.0605
-6 2 0 0.0997
3 1 -8 0.0432
-1 -8 0 0.0361
0 7 4 0.0403
0 1 -1 0.0239
0 0 0 0.0372
0 0 0 0.0410
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3A Se1A C1A . . 99.1(2) ?
C3A N1A C5A . . 108.9(3) ?
C3A N1A C4A . . 126.5(4) ?
C5A N1A C4A . . 124.6(3) ?
C3A N2A C10A . . 109.4(3) ?
C3A N2A C19 . . 127.2(3) ?
C10A N2A C19 . . 122.9(4) ?
Se1A C1A H1AA . . 109.5 ?
Se1A C1A H1AB . . 109.5 ?
H1AA C1A H1AB . . 109.5 ?
Se1A C1A H1AC . . 109.5 ?
H1AA C1A H1AC . . 109.5 ?
H1AB C1A H1AC . . 109.5 ?
N1A C3A N2A . . 108.6(3) ?
N1A C3A Se1A . . 124.8(3) ?
N2A C3A Se1A . . 126.5(3) ?
N1A C4A H4AA . . 109.5 ?
N1A C4A H4AB . . 109.5 ?
H4AA C4A H4AB . . 109.5 ?
N1A C4A H4AC . . 109.5 ?
H4AA C4A H4AC . . 109.5 ?
H4AB C4A H4AC . . 109.5 ?
C10A C5A N1A . . 107.4(4) ?
C10A C5A C6A . . 120.9(4) ?
N1A C5A C6A . . 131.7(4) ?
C7A C6A C5A . . 115.9(4) ?
C7A C6A H6A . . 122.0 ?
C5A C6A H6A . . 122.0 ?
C6A C7A C8A . . 122.4(4) ?
C6A C7A H7A . . 118.8 ?
C8A C7A H7A . . 118.8 ?
C9A C8A C7A . . 122.2(5) ?
C9A C8A H8A . . 118.9 ?
C7A C8A H8A . . 118.9 ?
C8A C9A C10A . . 115.4(4) ?
C8A C9A H9A . . 122.3 ?
C10A C9A H9A . . 122.3 ?
C5A C10A C9A . . 123.2(4) ?
C5A C10A N2A . . 105.7(4) ?
C9A C10A N2A . . 131.0(4) ?
C3B Se1B C1B . . 86(5) ?
Se1B C1B H1BA . . 109.5 ?
Se1B C1B H1BB . . 109.5 ?
H1BA C1B H1BB . . 109.5 ?
Se1B C1B H1BC . . 109.5 ?
H1BA C1B H1BC . . 109.5 ?
H1BB C1B H1BC . . 109.5 ?
C3B N1B C5B . . 116(4) ?
C3B N1B C4B . . 128(3) ?
C5B N1B C4B . . 116(4) ?
C3B N2B C10B . . 102(4) ?
C3B N2B C19 . . 132(3) ?
C10B N2B C19 . . 126(4) ?
N1B C3B N2B . . 108.1(18) ?
N1B C3B Se1B . . 125.1(18) ?
N2B C3B Se1B . . 127(3) ?
N1B C4B H4BA . . 109.5 ?
N1B C4B H4BB . . 109.5 ?
H4BA C4B H4BB . . 109.5 ?
N1B C4B H4BC . . 109.5 ?
H4BA C4B H4BC . . 109.5 ?
H4BB C4B H4BC . . 109.5 ?
N1B C5B C10B . . 97(5) ?
N1B C5B C6B . . 141(6) ?
C10B C5B C6B . . 122(2) ?
C7B C6B C5B . . 114(3) ?
C7B C6B H6B . . 122.9 ?
C5B C6B H6B . . 122.9 ?
C6B C7B C8B . . 123(3) ?
C6B C7B H7B . . 118.3 ?
C8B C7B H7B . . 118.3 ?
C9B C8B C7B . . 120(2) ?
C9B C8B H8B . . 119.8 ?
C7B C8B H8B . . 119.8 ?
C10B C9B C8B . . 117(2) ?
C10B C9B H9B . . 121.4 ?
C8B C9B H9B . . 121.4 ?
C9B C10B C5B . . 121(3) ?
C9B C10B N2B . . 122(6) ?
C5B C10B N2B . . 116(6) ?
Se2 C2A H2AA . . 109.5 ?
Se2 C2A H2AB . . 109.5 ?
H2AA C2A H2AB . . 109.5 ?
Se2 C2A H2AC . . 109.5 ?
H2AA C2A H2AC . . 109.5 ?
H2AB C2A H2AC . . 109.5 ?
C11 N3 C18 . . 108.9(3) ?
C11 N3 C23 . . 125.6(3) ?
C18 N3 C23 . . 125.0(3) ?
C11 N4 C13 . . 109.2(3) ?
C11 N4 C12 . . 126.8(3) ?
C13 N4 C12 . . 123.8(3) ?
C11 Se2 C2A . . 94.86(17) ?
N4 C11 N3 . . 108.8(3) ?
N4 C11 Se2 . . 126.9(3) ?
N3 C11 Se2 . . 124.2(3) ?
N4 C12 H12A . . 109.5 ?
N4 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
N4 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
N4 C13 C18 . . 106.6(3) ?
N4 C13 C14 . . 131.5(4) ?
C18 C13 C14 . . 121.9(4) ?
C15 C14 C13 . . 116.3(4) ?
C15 C14 H14 . . 121.9 ?
C13 C14 H14 . . 121.9 ?
C14 C15 C16 . . 122.1(4) ?
C14 C15 H15 . . 119.0 ?
C16 C15 H15 . . 119.0 ?
C17 C16 C15 . . 121.8(4) ?
C17 C16 H16 . . 119.1 ?
C15 C16 H16 . . 119.1 ?
C16 C17 C18 . . 115.7(4) ?
C16 C17 H17 . . 122.1 ?
C18 C17 H17 . . 122.1 ?
N3 C18 C13 . . 106.5(3) ?
N3 C18 C17 . . 131.3(3) ?
C13 C18 C17 . . 122.2(3) ?
C20 C19 C24 . . 122.5(3) ?
C20 C19 N2A . . 118.9(5) ?
C24 C19 N2A . . 118.6(5) ?
C20 C19 N2B . . 121(9) ?
C24 C19 N2B . . 115(8) ?
C19 C20 C21 . . 118.7(3) ?
C19 C20 H20 . . 120.7 ?
C21 C20 H20 . . 120.7 ?
C22 C21 C20 . . 120.5(3) ?
C22 C21 H21 . . 119.7 ?
C20 C21 H21 . . 119.7 ?
C21 C22 C23 . . 119.1(3) ?
C21 C22 H22 . . 120.5 ?
C23 C22 H22 . . 120.5 ?
C24 C23 C22 . . 121.9(3) ?
C24 C23 N3 . . 119.7(3) ?
C22 C23 N3 . . 118.4(3) ?
C19 C24 C23 . . 117.3(3) ?
C19 C24 H24 . . 121.3 ?
C23 C24 H24 . . 121.3 ?
O2 S1 O3 . . 115.94(19) ?
O2 S1 O1 . . 114.8(2) ?
O3 S1 O1 . . 114.0(2) ?
O2 S1 C25 . . 103.0(2) ?
O3 S1 C25 . . 104.2(2) ?
O1 S1 C25 . . 102.5(3) ?
F3 C25 F1 . . 108.3(5) ?
F3 C25 F2 . . 108.6(5) ?
F1 C25 F2 . . 106.9(5) ?
F3 C25 S1 . . 110.9(4) ?
F1 C25 S1 . . 111.3(4) ?
F2 C25 S1 . . 110.7(4) ?
F4 C26 F5 . . 104.9(5) ?
F4 C26 F6 . . 109.4(5) ?
F5 C26 F6 . . 107.1(4) ?
F4 C26 S2A . . 105.8(4) ?
F5 C26 S2A . . 116.0(4) ?
F6 C26 S2A . . 113.2(5) ?
F4 C26 S2B . . 119.5(4) ?
F5 C26 S2B . . 105.5(4) ?
F6 C26 S2B . . 109.7(4) ?
C27A C27A Cl1A 2_655 . 107.9(10) ?
C27A C27A H27A 2_655 . 110.1 ?
Cl1A C27A H27A . . 110.1 ?
C27A C27A H27B 2_655 . 110.1 ?
Cl1A C27A H27B . . 110.1 ?
H27A C27A H27B . . 108.4 ?
C27B C27B Cl1B 2_655 . 108.7(15) ?
C27B C27B H27C 2_655 . 110.0 ?
Cl1B C27B H27C . . 110.0 ?
C27B C27B H27D 2_655 . 110.0 ?
Cl1B C27B H27D . . 110.0 ?
H27C C27B H27D . . 108.3 ?
O4A S2A O5A . . 119.3(5) ?
O4A S2A O6A . . 108.6(5) ?
O5A S2A O6A . . 116.4(7) ?
O4A S2A C26 . . 107.6(5) ?
O5A S2A C26 . . 100.8(5) ?
O6A S2A C26 . . 102.0(5) ?
O5B S2B O6B . . 115.3(6) ?
O5B S2B O4B . . 113.1(5) ?
O6B S2B O4B . . 118.8(5) ?
O5B S2B C26 . . 107.5(5) ?
O6B S2B C26 . . 99.5(5) ?
O4B S2B C26 . . 99.5(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Se1A C3A . 1.891(4) ?
Se1A C1A . 1.946(4) ?
N1A C3A . 1.338(5) ?
N1A C5A . 1.386(5) ?
N1A C4A . 1.461(5) ?
N2A C3A . 1.339(5) ?
N2A C10A . 1.397(6) ?
N2A C19 . 1.439(4) ?
C1A H1AA . 0.9800 ?
C1A H1AB . 0.9800 ?
C1A H1AC . 0.9800 ?
C4A H4AA . 0.9800 ?
C4A H4AB . 0.9800 ?
C4A H4AC . 0.9800 ?
C5A C10A . 1.382(6) ?
C5A C6A . 1.404(6) ?
C6A C7A . 1.380(7) ?
C6A H6A . 0.9500 ?
C7A C8A . 1.393(8) ?
C7A H7A . 0.9500 ?
C8A C9A . 1.376(7) ?
C8A H8A . 0.9500 ?
C9A C10A . 1.391(7) ?
C9A H9A . 0.9500 ?
Se1B C3B . 1.89(2) ?
Se1B C1B . 1.94(2) ?
C1B H1BA . 0.9800 ?
C1B H1BB . 0.9800 ?
C1B H1BC . 0.9800 ?
N1B C3B . 1.337(19) ?
N1B C5B . 1.38(2) ?
N1B C4B . 1.455(18) ?
N2B C3B . 1.35(2) ?
N2B C10B . 1.40(2) ?
N2B C19 . 1.446(16) ?
C4B H4BA . 0.9800 ?
C4B H4BB . 0.9800 ?
C4B H4BC . 0.9800 ?
C5B C10B . 1.38(2) ?
C5B C6B . 1.41(2) ?
C6B C7B . 1.37(2) ?
C6B H6B . 0.9500 ?
C7B C8B . 1.40(2) ?
C7B H7B . 0.9500 ?
C8B C9B . 1.38(2) ?
C8B H8B . 0.9500 ?
C9B C10B . 1.38(2) ?
C9B H9B . 0.9500 ?
C2A Se2 . 1.961(4) ?
C2A H2AA . 0.9800 ?
C2A H2AB . 0.9800 ?
C2A H2AC . 0.9800 ?
N3 C11 . 1.352(5) ?
N3 C18 . 1.388(5) ?
N3 C23 . 1.444(5) ?
N4 C11 . 1.331(5) ?
N4 C13 . 1.391(5) ?
N4 C12 . 1.468(5) ?
Se2 C11 . 1.899(4) ?
C12 H12A . 0.9800 ?
C12 H12B . 0.9800 ?
C12 H12C . 0.9800 ?
C13 C18 . 1.392(5) ?
C13 C14 . 1.393(5) ?
C14 C15 . 1.376(7) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.405(7) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.391(6) ?
C16 H16 . 0.9500 ?
C17 C18 . 1.392(6) ?
C17 H17 . 0.9500 ?
C19 C20 . 1.382(5) ?
C19 C24 . 1.386(5) ?
C20 C21 . 1.389(5) ?
C20 H20 . 0.9500 ?
C21 C22 . 1.386(6) ?
C21 H21 . 0.9500 ?
C22 C23 . 1.387(5) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.387(5) ?
C24 H24 . 0.9500 ?
S1 O2 . 1.437(3) ?
S1 O3 . 1.437(3) ?
S1 O1 . 1.439(3) ?
S1 C25 . 1.821(5) ?
F1 C25 . 1.323(6) ?
F2 C25 . 1.328(6) ?
F3 C25 . 1.310(7) ?
F4 C26 . 1.301(6) ?
F5 C26 . 1.322(6) ?
F6 C26 . 1.333(6) ?
C26 S2A . 1.794(9) ?
C26 S2B . 1.850(8) ?
Cl1A C27A . 1.78(2) ?
C27A C27A 2_655 1.499(18) ?
C27A H27A . 0.9900 ?
C27A H27B . 0.9900 ?
Cl1B C27B . 1.81(3) ?
C27B C27B 2_655 1.52(3) ?
C27B H27C . 0.9900 ?
C27B H27D . 0.9900 ?
S2A O4A . 1.372(8) ?
S2A O5A . 1.415(8) ?
S2A O6A . 1.441(9) ?
S2B O5B . 1.430(8) ?
S2B O6B . 1.451(8) ?
S2B O4B . 1.500(7) ?